Comparison of H2 adsorption capacity of Bikitaite zeolite with reported values.
\r\n\t
",isbn:"978-1-83968-760-0",printIsbn:"978-1-83968-759-4",pdfIsbn:"978-1-83968-761-7",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"cc49d6034d85f8f2e2890c6acc3cc629",bookSignature:"Dr. Abhijit Biswas",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10285.jpg",keywords:"Mott Insulators, Semi Metals, Polycrystals, Single Crystals, Electronic Properties, Magnetic Properties, PLD, MBE, Topological Insulators, Topological Hall Effect, Devices Applications, Catalysis",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 9th 2020",dateEndSecondStepPublish:"October 7th 2020",dateEndThirdStepPublish:"December 6th 2020",dateEndFourthStepPublish:"February 24th 2021",dateEndFifthStepPublish:"April 25th 2021",remainingDaysToSecondStep:"5 months",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:"A pioneering researcher in the field of tailoring metal oxide crystal surfaces and growth as well as engineering of thin films for various emergent phenomena and energy applications. Dr. Biswas received his Ph.D. from POSTECH, South Korea.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"194151",title:"Dr.",name:"Abhijit",middleName:null,surname:"Biswas",slug:"abhijit-biswas",fullName:"Abhijit Biswas",profilePictureURL:"https://mts.intechopen.com/storage/users/194151/images/system/194151.png",biography:"Dr. Abhijit Biswas is a research associate at the Indian Institute of Science Education and Research (IISER) Pune, in India. His research goal is to design and synthesize highest quality epitaxial heterostructures and superlattices, to play with their internal degrees of freedom to exploit the structure–property relationships, in order to find the next-generation multi-functional materials, in view of applications and of fundamental interest. His current research interest ranges from growth of novel perovskite oxides to non-oxides epitaxial films, down to its ultra-thin limit, to observe unforeseeable phenomena. He is also engaged in the growth of high quality epitaxial layered carbides and two-dimensional non-oxide thin films, to exploit the strain, dimension, and quantum confinement effect. His recent work also includes the metal-insulator transitions and magneto-transport phenomena in strong spin-orbit coupled epitaxial perovskite oxide thin films by reducing dimensionality as well as strain engineering. He is also extremely interested in the various energy related environment friendly future technological applications of thin films. In his early research career, he had also extensively worked on the tailoring of metal oxide crystal surfaces to obtain the atomic flatness with single terminating layer. Currently, he is also serving as a reviewer of several reputed peer-review journals.\nDr. Biswas received his B.Sc. in Physics from Kalyani University, followed by M.Sc in Physics (specialization in experimental condensed matter physics) from Indian Institute of Technology (IIT), Bombay. His Ph.D., also in experimental condensed matter physics, was awarded by POSTECH, South Korea for his work on the transport phenomena in perovskite oxide thin films. Before moving back to India as a national post-doctoral fellow, he was a post-doc at POSTECH working in the field of growth and characterizations of strong spin-orbit coupled metal oxide thin films.",institutionString:"Indian Institute of Science Education and Research Pune",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"2",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"Indian Institute of Science Education and Research Pune",institutionURL:null,country:{name:"India"}}}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"20",title:"Physics",slug:"physics"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"205697",firstName:"Kristina",lastName:"Kardum Cvitan",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/205697/images/5186_n.jpg",email:"kristina.k@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"8356",title:"Metastable, Spintronics Materials and Mechanics of Deformable Bodies",subtitle:"Recent Progress",isOpenForSubmission:!1,hash:"1550f1986ce9bcc0db87d407a8b47078",slug:"solid-state-physics-metastable-spintronics-materials-and-mechanics-of-deformable-bodies-recent-progress",bookSignature:"Subbarayan Sivasankaran, Pramoda Kumar Nayak and Ezgi Günay",coverURL:"https://cdn.intechopen.com/books/images_new/8356.jpg",editedByType:"Edited by",editors:[{id:"190989",title:"Dr.",name:"Subbarayan",surname:"Sivasankaran",slug:"subbarayan-sivasankaran",fullName:"Subbarayan Sivasankaran"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"1591",title:"Infrared Spectroscopy",subtitle:"Materials Science, Engineering and Technology",isOpenForSubmission:!1,hash:"99b4b7b71a8caeb693ed762b40b017f4",slug:"infrared-spectroscopy-materials-science-engineering-and-technology",bookSignature:"Theophile Theophanides",coverURL:"https://cdn.intechopen.com/books/images_new/1591.jpg",editedByType:"Edited by",editors:[{id:"37194",title:"Dr.",name:"Theophanides",surname:"Theophile",slug:"theophanides-theophile",fullName:"Theophanides Theophile"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3092",title:"Anopheles mosquitoes",subtitle:"New insights into malaria vectors",isOpenForSubmission:!1,hash:"c9e622485316d5e296288bf24d2b0d64",slug:"anopheles-mosquitoes-new-insights-into-malaria-vectors",bookSignature:"Sylvie Manguin",coverURL:"https://cdn.intechopen.com/books/images_new/3092.jpg",editedByType:"Edited by",editors:[{id:"50017",title:"Prof.",name:"Sylvie",surname:"Manguin",slug:"sylvie-manguin",fullName:"Sylvie Manguin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3161",title:"Frontiers in Guided Wave Optics and Optoelectronics",subtitle:null,isOpenForSubmission:!1,hash:"deb44e9c99f82bbce1083abea743146c",slug:"frontiers-in-guided-wave-optics-and-optoelectronics",bookSignature:"Bishnu Pal",coverURL:"https://cdn.intechopen.com/books/images_new/3161.jpg",editedByType:"Edited by",editors:[{id:"4782",title:"Prof.",name:"Bishnu",surname:"Pal",slug:"bishnu-pal",fullName:"Bishnu Pal"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"72",title:"Ionic Liquids",subtitle:"Theory, Properties, New Approaches",isOpenForSubmission:!1,hash:"d94ffa3cfa10505e3b1d676d46fcd3f5",slug:"ionic-liquids-theory-properties-new-approaches",bookSignature:"Alexander Kokorin",coverURL:"https://cdn.intechopen.com/books/images_new/72.jpg",editedByType:"Edited by",editors:[{id:"19816",title:"Prof.",name:"Alexander",surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"1373",title:"Ionic Liquids",subtitle:"Applications and Perspectives",isOpenForSubmission:!1,hash:"5e9ae5ae9167cde4b344e499a792c41c",slug:"ionic-liquids-applications-and-perspectives",bookSignature:"Alexander Kokorin",coverURL:"https://cdn.intechopen.com/books/images_new/1373.jpg",editedByType:"Edited by",editors:[{id:"19816",title:"Prof.",name:"Alexander",surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"57",title:"Physics and Applications of Graphene",subtitle:"Experiments",isOpenForSubmission:!1,hash:"0e6622a71cf4f02f45bfdd5691e1189a",slug:"physics-and-applications-of-graphene-experiments",bookSignature:"Sergey Mikhailov",coverURL:"https://cdn.intechopen.com/books/images_new/57.jpg",editedByType:"Edited by",editors:[{id:"16042",title:"Dr.",name:"Sergey",surname:"Mikhailov",slug:"sergey-mikhailov",fullName:"Sergey Mikhailov"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"371",title:"Abiotic Stress in Plants",subtitle:"Mechanisms and Adaptations",isOpenForSubmission:!1,hash:"588466f487e307619849d72389178a74",slug:"abiotic-stress-in-plants-mechanisms-and-adaptations",bookSignature:"Arun Shanker and B. Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"878",title:"Phytochemicals",subtitle:"A Global Perspective of Their Role in Nutrition and Health",isOpenForSubmission:!1,hash:"ec77671f63975ef2d16192897deb6835",slug:"phytochemicals-a-global-perspective-of-their-role-in-nutrition-and-health",bookSignature:"Venketeshwer Rao",coverURL:"https://cdn.intechopen.com/books/images_new/878.jpg",editedByType:"Edited by",editors:[{id:"82663",title:"Dr.",name:"Venketeshwer",surname:"Rao",slug:"venketeshwer-rao",fullName:"Venketeshwer Rao"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"4816",title:"Face Recognition",subtitle:null,isOpenForSubmission:!1,hash:"146063b5359146b7718ea86bad47c8eb",slug:"face_recognition",bookSignature:"Kresimir Delac and Mislav Grgic",coverURL:"https://cdn.intechopen.com/books/images_new/4816.jpg",editedByType:"Edited by",editors:[{id:"528",title:"Dr.",name:"Kresimir",surname:"Delac",slug:"kresimir-delac",fullName:"Kresimir Delac"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"26735",title:"Surgical Prevention of Arm Lymphedema in Breast Cancer Treatment",doi:"10.5772/25163",slug:"surgical-prevention-of-arm-lymphedema-in-breast-cancer-treatment",body:'Disruption of the axillary nodes and closure of arm lymphatics can explain the significantly high risk of early and late lymphatic complications after axillary dissection, especially the most serious complication that is arm lymphedema which occurs in about 25% (ranging from 13 to 52%) of patients. Sentinel lymph node (SLN) biopsy has reduced the severity of swelling to nearly 6% (from 2 to 7%) and, in case of positive SLN, complete axillary dissection (AD) is still required. That is why ARM method was developed aiming at identifying and preserve lymphatics draining the arm. It consists in injecting intradermally and subcutaneously a small quantity (1-2 ml) of blue dye at the medial surface of the arm which helps in locating the draining arm lymphatic pathways. ARM technique allowed to find variable clinical anatomical conditions from what was already generally known, that is the most common location of arm lymphatics below and around the axillary vein. In about one-third of the cases, blue lymphatics can be found till 3-4 cm below the vein, site where SLN can easily be located, justifying the occurrence of lymphedema after only SLN biopsy. ARM procedure showed that blue nodes were almost always placed at the lateral part of the axilla, under the vein and above the second intercostals brachial nerve. Leaving in place lymph nodes related to arm lymphatic drainage would decrease the risk of arm lymphedema, but not retrieving all nodes, the main risk is to leave metastatic disease in the axilla. Conversely, arm lymphatic pathways when they enter the axilla, cannot be site of breast tumoral disease and their preservation would certainly bring about a significant decrease of lymphedema occurrence rate (1-4).
Another important aspect to point out is that, in the axilla, new lymphatic vessel formation (lymphangiogenesis) occurs in response to the ligation of lymphatic vessels involved in lymph node retrievement. Lymphangiogenesis and lymphatic hypertension were demonstrated experimentally in case of lymphatic drainage obstruction. And, in response to lymphatic hypertension, lympho-venous shunts open and provide alternative lymphatic pathways when the main ones are obstructed. These mechanisms represent an adaptive response to lymphatic hypertension but are not enough to restore normal flow parameters. Furthermore, chronic obstruction to lymph flow progressively leads to a reduced lymphatic contractility, lymphatic thrombosis and fibrotic changes, at a different degree according to variable constitutional predisposition (5-9)
Recent advances in the treatment of breast cancer, specifically as concerns the prevention of lymphatic complications following sentinel lymph node biopsy and axillary dissection brought to the proposal of a new technique to primarily prevent lymphedema by microsurgical lymphatic-venous anastomoses. ARM technique allows to identify arm lymphatics and lymph nodes which can therefore be preserved even though there is the risk to leave undetected metastatic disease in the axilla. But, it is almost impossible to preserve efferent lymphatics from the blue nodes because they join the common axillary nodal basin draining the breast. Thus, not preserving efferent lymphatics makes practically impossible to preserve arm lymphatic flow. So, on the basis of our wide experience in the treatment of lymphedema by microsurgical lymphatic-venous anastomoses (LVA), we thought to perform LVA immediately after finishing nodal axillary excision. The surgical technique proposed for patients with operable breast cancer requiring an axillary dissection consisted in carrying out LVA between arm lymphatics identified by injecting blue dye in the arm and an axillary vein branch simultaneously (Lymphatic Microsurgical Preventive Healing Approach – LY.M.P.H.A.) (10). It is almost always possible to find blue lymphatics and also to find a vein branch long enough to be connected to arm lymphatics which are usually locate very laterally.
Patients are followed up both clinically by volumetric assessment and by lymphangioscintigraphy performed before surgery and after 18 months. Blue nodes in relation to lymphatic arm drainage can be identified in almost all patients after blue dye injection at the arm. All blue nodes must be resected and 2 to 4 main afferent lymphatics from the arm can be prepared and used for anastomoses. Lymphatics are introduced inside the vein cut-end by a U-shaped stitch. Other few stitches are given to fix the lymphatic adventitia to the vein wall. The operation takes only 15-20 minutes averagely, since both lymphatics and the vein are prepared during nodal dissection. LVA proved not only to prevent lymphedema but also to reduce early lymphatic complications (i.e. lymphorrhea, lymphocele) thanks to the reduced regional intralymphatic pressure. Drain tubes can be removed after about 7-10 days at the utmost. Post-op lymphangioscintigraphy allowed to demonstrate the patency of microvascular anastomoses after over 1 year and half from operation.
Study design
Among fortynine consecutive women from March 2008 to September 2009 addressed to complete AD, performed by surgeons of the same Beast Unit, who used the same technique, 46 were randomly divided in two groups, the other 3 were not analyzed because refused to perform lymphoscintigraphy (LS) pre-operatively. Twentythree underwent LYMPHA technique, performed by a surgeon skilled in lymphatic microsurgery, for the prevention of arm lymphedema (LYMPHA group – LG). The other 23 patients had no preventive surgical approach (control group – CG). No wrapping neither compression therapy was used in any of the patients of both groups.
The average age was 57 years (range 39-80 years). In order to be included in this prospective study, patients with unilateral breast cancer had to be addressed to complete AD due to clinically or ultrasonographic positive axillary limph nodes or positive SLN. Exclusion criteria were cases in whom only SLN biopsy technique was performed and SLNs were negative.
In the LYMPHA group (LG), 16 patients there were lymph nodal metastasis and therefore lymphatic venous anastomosis were performed during the primary surgery together with breast cancer treatment, sentinel lymph node biopsy, intraoperative frozen sections (showing the metastasis) and axillary dissection (AD). In other 7 patients there were no lymph nodal metastasis demonstrated by intraoperative frozen sections and therefore LYMPHA technique was planned after finding micrometastasis by following immunohistochemical investigations. Thus, in this last group of patients we could perform LYMPHA during the complete lymph nodal dissection in the second time surgery.
Operating technique
Patients signed a specific consent form indicating the kind of operation, possible risks, and complications to participate or not in the LYMPHA procedure. The blue dye (Lymphazurin) was injected in the volar surface of the upper third of the arm in a quantity of about 1-2 ml intradermally, subcutaneously and under muscular fascia. Usually after 5-10 minutes it is already possible to visualize arm blue lymphatics. Axillary nodal dissection was performed usually starting far from the upper lateral part of the axilla which was removed nearly at the end of the dissection in order not to damage the lymphatic pathways coming from the arm. This lymphatics were temporally clipped near their afference to the nodal capsule and thus prepared for anastomosis.
During lymph nodal dissection also one or two collateral branches of the axillary vein are prepared with a length suitable for reaching the lymphatic vessels. The microsurgical technique of lymphatic venous anastomosis has already been described (11). The vein was averagely 2 mm in diameter and lymphatics about half mm. the number of lymphatics anastomosed varied from 2 to 4. The technique is the “sleeve” procedure: lymphatics are put into the vein cut-end. A collateral of the axillary vein is used for anastomoses. In some cases a big gap inbetween the vein and the lymphatics can be found, but in these cases it is usually enough to better dissect the vein and above all the lymphatics from the surrounding tissues. In case it is necessary one of the subscapular or thoraco-dorsal veins which are usually long enough can also been used. A particular attention must be paid in placing the drain tube in order not to damage the anastomosis (Fig.1). Lymphatic-venous anastomoses take only 15-20 minutes to be performed and in our study were performed by a surgeon skilled in lymphatic microsurgery. There is no increased rate of blood loss, wound infection and seromas compared to standard ALND (Fig. 2).
Clinical and lymphoscintigraphic assessment
All patients of the two groups were preoperatively studied clinically by volume measurements (using the formula of a truncated cone according to Kuhnke method) (10) and by lymphoscintigraphy. Lymphedema, was defined as a difference in excess volume of at least 100 ml compared to preoperative VOL measurements. The follow up included volumetry at 1, 3, 6, 12 and 18 months postoperatively in both groups.
Lymphoscintigraphy was carried out in 21 cases in the LG and in 20 cases of the CG after 18 months postoperatively (Fig. 3).
Lymphatic-venous-anastomoses (rectangle) to prevent arm lymphedema (LYMPHA). Note the blue dye (*) injected at the upper third of the volar surface of the arm to visualise arm lymphatics. The patency of lymphatic-venous anastomosis is proved by the passage of the blue dye into the vein branch (arrow).
Patient who underwent axillary lymphnodal dissection and primary surgical prevention of secondary lymphedema by LYMPHA procedure.
Statistical analysis
Non-parametric tests were used to explore the variable relationships between groups and between timing. The comparison between groups of quantitative variables age, BMI, Preop LS, lymphonodes retrived, metastatic lymphnodes (MLS LN) and volume at baseline was performed using Wilcoxon test. Nominal baseline variables surgical procedure, radiotherapy and presence of cellulitis were compared using Chi square or Fisher’s Exact Test.
The comparison of difference between baseline and volume after 1, 3, 6, 12 and 18 months from operation in LG and CG was performed using Wilcoxon test (between groups) and matched pair test (between timing). The volume difference between baseline and different timing in LG and CG was represented by box plots showing 10 , 25 , 75 and 90 percentiles. Number of patients with lymphedema, defined as a difference in excess volume of at least 100 ml, at 18 months in PG and CG were compared using 2-sided Fischer’s Exact Test.
Results
Lymphedema appeared in 1 patient in the LG after 6 months from the operation (4,34 %) and persisted till 18 months later. It occurred in a patient who underwent radiotherapy and became stable with time without any inflammatory complications. In the CG lymphedema occurred in 7 patients (30,43 %) and appeared mostly after 3 months from operation.
Lymphoscintigraphic patterns before and after axillary lymphnodal dissection associated with LYMPHA technique.
Beginning from month 3, the proportion of patients with lymphedema was statistically higher in CG (p-value=0.047). Table 1 summarizes baseline characteristics of all participants, according to treatment group. There were no significant differences between the two groups in the baseline values of measures of demographic and anthropometric data, in disease characteristics and in type of surgery, and in the proportion of women who undertook to radiotherapy and had a cellulitis. In Figure 4, volume difference between baseline and different timing in LG and CG is represented by box plots showing 10 , 25 , 75 and 90 percentiles.
When compared with previous volume measure, no significant difference in the arm volume were observed in LG during follow-up, while the arm volume in CG showed a significant increase after 1 (mean difference 11.61 ml, S.E. 3.87, p-value<0.01), 3 (mean difference 22.82 ml, S.E. 5.9, p-value<0.01) and 6 months (mean difference 31.56 ml, S.E. 5.78, p-value<0.01) from operation. No significant changes in arm volume were observed at month 12 and 18, in comparison with data registered at month 6 and 12, respectively, in CG. Significant higher volume with respect to baseline after 1, 3, 6, 12 and 18 months from operation (every timing p-value<0.01) was detected in CG in comparison with LG.
Duplex scan allowed to exclude a venous pathology in all patients. LS allowed to confirm the lymphostatic nature of the edema. To quantify visual findings in LS, the Kleinhans transport index (TI) was used (4,13,14). The TI includes the following parameters: transport kinetics (K), distribution of the tracer (D), appearance time of lymph nodes in minutes (T), visualization of lymph nodes (N), visualisation of lymph vessels (V); TI = K + D + (0,04 x T) + N + V (Table 2). Normal lymphoscintigraphy pattern corresponded to TI less than 10. An impaired LS pattern in our study had a mean TI of 16 (range 12-19).
Moreover, pre-operatively LS had a significant predictive value (TI) in terms of risk of lymphedema appearance. To this regard LS proved to be an instrumental criteria to select patients at risk for secondary lymphedema.
Post-operatively LS demonstrated the patency of microlymphaticvenous anastomosis (patency rate: 95,6%) both through direct (visualization of preferential lymphatic pathway, disappearance of the tracer passing into the blood stream) and indirect (early liver uptake of the tracer) parameters in the LG group. In the CG on the other hand LS allowed to point out lymphatic drainage impairment in patients with secondary lymphedema.
Notwithstanding the wide variability in lymphedema prevalence, the incidence of secondary arm lymphedema is significant. Sentinel lymph node biopsy (SLNB) was introduced and carried out to prevent lymphedema but, recent studies demonstrated that even with SLNB alone lymphedema rates are not negligible (13,17).
Therefore, prevention is of key importance to avoid lymphedema occurrence.
Axillary Reverse Mapping (ARM) procedure represents an attempt to identify and preserve arm lymphatic drainage. Success of this technique in preventing lymphedema will require ongoing follow-up and studies (6). Blue nodes were always located in the same position, at the lateral part of the dissection, under the axillary vein and just above the second intercostal brachial nerve (7). The main issue remains to make sure that the nodes identified are not metastatic and can be preserved during AD. Since the lymphatic pathways from the arm cannot be involved by metastatic process of the primary breast tumor, its preservation should not imply any risk of leaving undetected diseases in the axilla (1). With ARM technique the detection rate of blue lymphatics and nodes is 61-71%, and the preservation rate of 47% (1,6,7). The question is: can we spare what we find? The identification of afferent lymphatics and nodes belonging to the arm lymphatic pathways appears feasible. Nevertheless, the identification of the efferent lymphatics, which is mandatory to truly preserve the lymphatic flow of the arm, is almost impossible since the lymphatics departing from the blue nodes join the common lymphatic pathways draining the breast. Therefore, the preservation is practically impossible. That’s why we conceived and carried out LYMPHA technique, which consist in performing LVA between arm lymphatics and collateral branches of the axillary vein at the same time as AD. Lymphatic-venous anastomoses are performed at the upper lateral part of the axilla, thus somehow protected from the negative effect of postop radiation. In fact, postop radiation did not cause any relevant problem in the patients with lymphatic-venous anastomoses in this study. Only in two patients, a transitory (for 3 and 5 days respectively) slight arm edema was observed which disappeared spontaneously. Patients were followed by volume measurements which allowed to demonstrate the absence of any negative effect of postop radiation. Furthermore, postop lymphoscintigraphy proved the patency of anastomoses long after surgery and radiation. The preservation of arm lymphatics carries no risk of leaving disease in the axilla undetected, and it permits the prevention of lymphedema (10). Patients candidate for LYMPHA are those one addressed to AD with either clinical axillary N+ or SLN+. In pre-operative patients selection for LYMPHA clinical and instrumental criteria were evaluated (Fig.4).
Clinical and instrumental criteria to select patients for LYMPHA technique
History and physical esamination of the patients, together with BMI, could allow to select patients at risk for lymphedema and this suspect could be confirmed by LS, using semiquantitative evaluation which is represented by TI (15-19). Preop lymphoscintigraphy is useful to select patients at risk for arm lymphedema. LS shows lymphatic impairment (in terms of transport index) compared to the contralateral arm already present pre-operatively.
The quality of life is gaining more and more importance thanks to the prolongation of survival brought about by advanced and combined treatment of different tumors. Surgery has to be more and more conservative and try to maintain organ function and reduce morbility. LYMPHA technique proved to represent a new strategy of treatment to reduce morbility of axillary lymph nodal dissection when it is not possible to preserve arm lymphatic pathways due to the risk to leave tumoral diseases correlated to the breast cancer.
Gas separation and storage processes are essentially important to various aspects in human society, such as energy consumption, environmental security, and industrial production. Energy and environmental concerns are currently at the forefront of global attention. So, carbon dioxide separation is crucial to the mitigation of greenhouse effect [1, 2, 3]. Besides, separation of hydrogen and methane together with storage is indispensable for the prevalent use of clean energy. In the case of toxic gases, the separation and storage of ammonia and carbon monoxide are important for pollution control and the synthesis of industrial chemicals. The conventional gas separation technologies such as pressure swing adsorption (PSA), cryogenic distillation, etc. are very energy intensive as well as capital intensive. Also separation methods like liquid adsorbent are cost-effective. In the distillation process, the repeated evaporating-condensing cycle of the mixture under harsh conditions is a problematical job. Also generation of liquid adsorbent is a main concern which required the heating and cooling of massive solvent medium to release adsorbed gas. Due to these negative aspects, the potential of emerging technologies based on adsorption or membrane separations is highly amiable alternative process and has been proposed as more energy-efficient technologies [4, 5, 6, 7, 8]. According to existing literatures, membrane-based separation technology only consumes 10% energy of that for distillation [9]. From the industrial perspective of storage and separation of different gases, adsorption-based technique is more amicable and commendable due to its superiority to other techniques like simplicity of design, easy operation, and low cost. The separation efficiency relies on internal porosity and surface properties of solid adsorbent due to their key role in gas sorption. Alternatively, molecular properties of the adsorbent such as chemical affinity or molecular size of the separated components play a vital role in the separation process. Separation and purification, meanwhile, involve the selective adsorption of particular species from gas mixtures. Also, gas storage requires elevated pressures due to volumetric capacity considerations of porous materials and the need to deliver gas at ambient pressure or above.
\nNanoporous materials have attracted huge interest among the communities of materials science, chemical engineering, and chemistry due to their excellent properties such as high surface area, large pore volume, and specific surface chemistry. The term nanoporous refers to any material with a pore size below ~100 nm. According to the International Union of Pure and Applied Chemistry (IUPAC) guidelines, nanoporous materials encompass both the microporous (<2 nm) and mesoporous (2–50 nm) regimes. As per literature data, porous materials like zeolites, carbon, aluminophosphates, carbon nanotubes, silica gel, pillared clays, inorganic and polymeric resins, MOFs, and MOFs composites have been investigated as adsorbents. In industry some of the adsorbents are now used for different applications. In the literature, relevant reviews and monographs have discussed the syntheses process, characterizations, and the adsorption properties of these porous materials [9, 10, 11, 12, 13, 14]. The importance of porous materials for different application is summarized in the literature, which can be helpful for the next-generation researcher. Among all porous material, especially in the microporous family, zeolites are the first and foremost emerging materials and attracted increasing interest because of their unique physical and chemical properties, such as high surface area, high chemical resistance, extraordinary mechanical properties, good adsorption, and catalytic properties due to specific surface chemistry [15, 16, 17, 18, 19, 20, 21, 22]. These peculiar and amazing properties have highlighted the potential of this material in a variety of applications and particularly in the area of gas separation and storage application [23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34]. Zeolites are traditionally referred to as a family of open-framework aluminosilicate materials consisting of orderly distributed micropores in molecular dimensions. Topologically, zeolites are three-dimensional networks of corner-sharing tetrahedral TO4 (“T” denotes tetrahedrally coordinated Si, Al, or P), and different ways of tetrahedra connection lead to a diversity of zeolite framework types based on various compositions [35]. Silica zeolites consist of four-coordinated Si bridged by oxygen atoms [36]. To date, 235 distinct zeolite framework types have been identified in natural or synthetic zeolites, each of which has been assigned a three-letter code by the International Zeolite Association (Figure 1) [37].
\nFramework types of different zeolites [36, 37].
For zeolite synthesis, the well-known conventional hydrothermal method is a widely used technique. Besides the other synthesis method like sonochemical and sonochemical-assisted hydrothermal method, microwave-assisted methods are more popular and advanced synthesis process to achieve phase pure high-quality zeolites in terms of their shape, size, porosity, uniform structure, and better crystallinity [38]. Furthermore, for the synthesis of zeolite membrane on the porous support, the in-situ and ex-situ (secondary growth) hydrothermal techniques are the well known process and more popular among other synthesis routes. In the case of in situ hydrothermal process, the porous support is immersed into the synthesis solution, and the membrane layer is formed directly through direct crystallization in a suitable time period. But in this process, the probability of attaining the high-quality membrane on the support is less. So ex situ hydrothermal method which is also known as seeded growth technique is an effective and accepted approach towards the development of better membrane on the support surface. This method has potential advantages in terms of achieved preferential orientation control of membrane microstructure and higher reproducibility if compared with the in situ synthesis method [39]. Extensive studies have been performed aiming at investigating potential of zeolites and derived membranes for gas separation [40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56]. Specific zeolites have a high capacity and selectivity for the gases of interest, leading to compact and efficient separation/storage systems.
\nTo make this book chapter comprehensive, here three different types of zeolitic material were focused. The first one is siliceous deca-dodecasil 3R (DDR) zeolite which has elliptical pore openings defined by 8-member ring windows with an effective size of 0.36 × 0.44 nm2, and it is useful for separation of small-sized gas [27, 43, 50]. Another important zeolite is silicoaluminophosphate (SAPO 34). SAPO 34, a chabazite zeolite with a composition of SixAlyPzO2, where x = 0.01–0.98, y = 0.01–0.60, and z = 0.01–0.52, has an average pore size of 0.38 nm and plays an important role for gas separation application [32]. The last one is Bikitaite (BIK) zeolite having a unit cell chemical composition Li2(Al2Si4O12)-2H2O [11, 36]. It is a small pore (diameter 0.28–0.37 nm) sized zeolite and has been studied for various applications and most notably has shown better performance in gas separation and storage application. The detail synthesis protocol and techniques used to synthesize zeolites and high-quality membrane have been discussed here. After all, the performance of the developed materials was discussed elaborately for better understanding and presents the future aspect of these materials.
\nThe chemical reagents used are boehmite powder (SASOL, Germany), colloidal silica (Ludox HS- 30, Sigma Aldrich), structure directing agent (SDA) 1-adamantanamine (Sigma Aldrich), ethylene diamine (Merck, Mumbai, India), LiOH flakes (Merck, India), phosphoric acid (Qualigens fine chemicals, India), morpholine (S. D. fine chemicals, India), and deionized water.
\nThree unlike zeolites were synthesized by three different techniques like sonochemical, sonochemical-assisted hydrothermal method, and simple hydrothermal route. In the case of synthesis of the DDR zeolite, the sonochemical synthesis approach was implemented which is assisted by the complete growth of DDR crystal in a shorter crystallization time. The precursor solution containing the molar ratio of 1 silica:0.5 1-adamantanamine:4 ethylene diamine:100 water was used in the synthesis of the DDR crystals. The details of step-by-step synthesis process for DDR zeolite was already described in the previously reported work [40]. Two different mixtures were prepared. It is reported that first the measured amount of Ludox and water were mixed together (mixture-1). Then in another mixture (mixture-2), the ethylene diamine and water were mixed in a beaker followed by addition of 1-adamantanamine. Then the final mother sol (mixture 1 + mixture 2) was sonicated for 1 h. For fast synthesis of DDR zeolite, the ultrasound equipment (UIP1500 hd HIELSCHER Ultrasound Technology) which produces acoustic waves at frequency of 20 kHz was very useful [28]. The energy input for sonication was 250 W, and the mother sol was kept for aging for 1–9 days after sonication. The powdered products were recovered through centrifugation, washed with DI water until pH < 8, and then dried in the oven at 100°C for further characterization.
\nIn the case of Bikitaite zeolite, the molar composition of the sol used for the synthesis was 10 Li2O:0.5 Al2O3:2.5 SiO2:600 H2O [56]. Like the previous protocol, two reactant mixtures were prepared respectively by suspending the measured amount of colloidal silica and lithium hydroxide in deionized water (DI water) in a glass beaker (mixture 1). Mixture 2 was prepared by adding the measured amount of boehmite in lithium hydroxide. Then it was mixed slowly to mixture 1 with constant and vigorous stirring, and the mixture turned into a milky white sol. The resulting mixture was sonicated for 3 h. The energy input of sonication was varied from 150 to 250 W, followed by aging for 72 h. Then the sonicated mixture was poured into Teflon-lined stainless steel autoclave. Hydrothermal crystallization was continued under autogenous pressure in a hot air oven at 100°C for 24 h. For comparison, the different Bikitaite samples were synthesized by hydrothermal process similar to the abovementioned condition without sonication treatment. After synthesis, the zeolite powders were washed thoroughly with deionized water until the pH of the washing liquid became neutral and then dried at room temperature for further characterization.
\nThe molar composition of the sol used for the SAPO 34 zeolite synthesis was Al2O3:SiO2:P2O5:H2O 1:0.3:1:66. In a typical synthesis, first boehmite powder, phosphoric acid, and the required amount of water were mixed properly by using the stirrer with 600 rpm. The mixture was stirred overnight (mixture 1). Another mixture was prepared by dissolving the calculated amount of silica sol, morpholine, and deionized water (mixture 2). Then the reaction mixture was added slowly with mixture 1, and the resulted mother solution was stirred for another 1 hour at room temperature. The resulting mixture was stirred vigorously for 15–30 min and was kept stirring overnight to produce a homogeneous sol. The prepared homogeneous sol was kept in an autoclave, and the reaction was started at 170°C for 120 h. Finally the zeolite powders were centrifuged at 12,000 rpm for 20 min followed by washing with distilled water and the same washing process repeated four times. The resultant precipitate was dried in the oven at 100°C for 1 h.
\nAn indigenous clay-Al2O3 tube of diameter 10 mm, thickness 3 mm, and 60 mm length was used as support for synthesis of the membrane. The membranes were synthesized by secondary growth hydrothermal techniques. In this technique, first the seed layer was applied on the support by using different intermediate layer in order to attach the seed crystal and prepare a uniform seed layer on the support. Then the membranes were synthesized by secondary growth of the seed layer by hydrothermal process. The membrane synthesis procedure for SAPO 34, DDR, and Bikitaite zeolites was discussed in details in our previous work [47, 50, 56].
\nThe crystalline structure of the as-synthesized zeolites and membranes was determined by XRD patterns. XRD was carried out on a Philips 1710 diffractometer using CuKα radiation (α =1.541° A). The characteristic vibration bands for zeolite powders were investigated by FTIR (Nicolet 5PC, Nicolet analytical instrument, Madison, WI). Thermogravimetric analyses (TGA) and differential thermal analyses (DTA) were performed in static air using the thermogravimetric analyzer (NETZSCH STA 409 C F3 Jupiter, Germany). The samples were heated at a rate of 10°C min−1 under air flow. The N2 adsorption/desorption measurements of different zeolite powder were evaluated on a volumetric gas adsorption analyzer (autosorb-iQ-MP, Quantachrome) at 77 K. The sample used in the adsorption measurement was degassed at 423 K for 6 h before the measurements. Pore size distributions and surface area data of the synthesized powders were collected from N2 adsorption at 77 K. The same apparatus was also used for the measurement of H2 adsorption/desorption isotherms at 77 K up to 1 bar. Prior to adsorption study, the sample was out-gassed appropriately at 250°C for 24 h under high vacuum (106 mbar). In this case, He (99.999%) and N2 (99.999%) were used as carrier gas. Accessible microporous volume has been estimated by using the Dubinin-Radushkevich (DR) method. Transmission electron microscopy (TEM) measurements were carried out with a Tecnai G2 30ST (FEI) operating at 300 kV. The microstructure, elemental mapping with EDAX, and cross-sectional line scanning of the synthesized membranes were examined using field emission scanning electron microscopy (FESEM: model Leo, S430i, UK). X-ray photoelectron spectroscopy (XPS) measurements of support, chemically modified support, and respective membrane were carried out on an XPS system (PHI 5000 VersaProbe II, ULVAC-PHI, INC., USA) using a monochromatic Al Kα X-ray source (1486.6 eV). To identify the bonding between seed crystal and support surface, Raman analysis was carried by Raman microscope (RENISHAW inVia, UK).
\nThe gas permeation experiment was done by a specially designed permeation cell where the membrane was mounted in a stainless steel permeation cell and sealed by silicone O-rings. Prior to permeation experiment, the leak test was carried out in order to obtain the correct data. The complete description of gas permeation measurement is given in the supporting information of our published paper [40].
\nSiliceous deca-dodecasil 3R (DDR) zeolite has elliptical pore openings defined by 8- member ring windows with an effective size of 0.36 × 0.44 nm, and it is useful for separation of smaller-sized gas. DDR zeolites were synthesized by sonochemical method without the application of hydrothermal treatment. It is prepared only under sonication energy at different aging time ranging from 2 to 5 days. Figure 2 shows all the characterization results of DDR zeolite obtained from XRD, IR, and FESEM. The XRD results of the sample explained the crystalline pattern, and the characteristic peaks are calculated by their (hkl) values. The acquired XRD patterns of the sample are most similar to that of the DDR structure, and the d-values are in agreement with those reported literature data [27]. The intensity and peak positions are well matched with the reported XRD patterns which explained the crystalline nature of the nanosized DDR zeolite. In the XRD pattern of sample aging for 2 and 3 days as shown in Figure 2(a), the intensity increased gradually, and it confirms the more crystalline nature of the synthesized DDR zeolite (aging sample for 3 days).
\n(a) XRD patterns of DDR seed crystals synthesized for 2 days (lower), 3 days (middle), and 5 days (top); (b) IR spectrum of DDR zeolite synthesized for 5 days; and (c) corresponding FESEM image [43, 50].
\nFigure 2(b) shows the IR result of DDR crystals, and the strong vibration was noticed at 1377, 883, 767, 647, and 437 cm−1. The characteristic band at 437 and 767 cm−1 was assigned to O–T–O (T = Si) bending and Si–O tetrahedral vibration, respectively. Here, more importantly the appearance of the peaks at 647 cm−1 was attributed to the double ring external linkage. The peaks at about 2915 and 2860 cm−1 correspond to the stretching vibration of 1-adamantanamine [44]. The symmetric stretching vibration of internal tetrahedron was shown at 747 cm−1. Figure 2(c) shows the FESEM image of DDR zeolite, and elemental analysis showed that the desired atomic ratio of the DDR zeolite was obtained after 5 days of synthesis. The FESEM micrograph showed that the synthesized DDR seeds are nanosized powder having size 20 nm. The surface area of the synthesized powder was 212 m2 g−1. In sonochemical reaction process, free radicals are formed due to evolution of huge energy during collapsing of bubbles. It activates the reaction species which assisted in the nucleation and growth of colloidal nanoparticles of the reaction products [45]. In conventional synthesis process, the time required for complete reaction process is more which is often several days. But in sonochemical process, it needs less time for complete reaction process. From the XRD results, it can be assumed that the effect of sonication reduced the reaction time and formed crystalline DDR zeolite. The shortened reaction time is attributed to an extremely high temperature at the interface between a collapsing bubbles and the bulk solution [45]. The mass transport as well as hydrolysis and condensation reaction which were responsible for zeolite formation is controlled in this whole process. For detail, reaction mechanism and explanation in favor of this result were discussed elaborately in our reported work [42].
\nTo develop a continuous zeolite membrane on the support surface, at first the coverage of the seed particles must be high. Generally, polycrystalline zeolite membrane contains defects (non-zeolitic pores) which are larger than zeolitic pores. The formation of non-zeolitic pores resulted from cracks and defects of the membrane layer. The non-zeolitic pores are mainly responsible for decreasing the selectivity. So in order to form a better membrane, initially seed layer plays a major role, and the adherence with the support layer is pretty much important. The lack of proper adherence of seed crystals with support may initiate the crack formation in the membrane layer. For this, different types of polymeric coating layer were used as intermediate linker between seed layer and support. The reason behind the selection of different intermediate layer and the detail mechanism were described in the literature [40, 46, 47, 50]. In the case of DDR zeolite membrane synthesis, the polymer polydiallyldimethylammonium chloride (PDADMAC) was used as intermediate linker.
\nPDADMAC is a high charge density homopolymer, and it can interact with several solid materials having negative surface charges. As an effect, the PDADMAC adsorbs on the alumina support primarily via electrostatic attraction between the negatively charged clay-Al2O3 support and the positively charged PDADMAC. Also the PDADMAC polymer can bind the negatively charged DDR zeolite particles by electrostatic attraction. As per the binding mechanism, it is assumed that due to electrostatic interaction, the negatively charged DDR zeolite particles were formed homogeneously and easily deposited on the modified support surface. This may facilitate the formation of a uniform and dense zeolite DDR membrane on the support surface. Figure 3 shows the schematic outlook of the binding mechanism of zeolite seed layer on the support surface via using PDADMAC as intermediate linker.
\nSchematic of the binding mechanism between zeolite seed crystals and the support surface via PDADMAC polymer as an intermediate linker [50].
The surface morphology and cross-sectional view of the synthesized DDR zeolite membrane are shown in Figure 4(a) and (b). From the images, it can be assumed that a well-crystalline highly interlocked membrane layer was formed on the support having a uniform thickness of about 20–25 μm. Also, the phase purity of the DDR zeolite was confirmed from EDAX analysis (inset of Figure 4(a)), and it shows the atomic ratio of the Si and O is 1:2 which is desirable for DDR formation. The corresponding line scanning view (Figure 4(c) and (d)) throughout the membrane layer and support surface explained that the uniform membrane layer is formed on the support surface only and there is no penetration of zeolite layer into the support surface. For this outcome, intermediate PDADMAC plays a vital role. Regarding the development of continuous membrane formed or not on the support was indicated by FESEM and XRD results. But the actual quality of the zeolite membrane can only be evaluated by gas permeation properties of the membrane.
\nFESEM images of (a) DDR membrane on the PDADMAC-modified support with EDAX data (as inset), (b) cross-sectional view of DDR membrane layer indicating the thickness by the arrow, (c) line scanning through the support and membrane layer with compositional element scan, and (d) the corresponding spectra of O, Al, and Si (distance in micron) [50].
In the case of SAPO 34 zeolite membrane, a number of studies and effort have been carried out to develop a high-quality defect-free membrane. In the literature a lot of work has been done on SAPO 34 zeolite for gas separation and storage application [32, 33, 34]. In our work an effort has been given to improvise the membrane structure and minimize the defects by different techniques for targeting the higher separation efficiency. SAPO 34 is a small pore zeolite (pore diameter of 0.38 nm), and it has a chabazite (CHA) type framework which is a promising member of the zeolite family. This interesting and efficient material has been studied for various applications. But notably its performance towards hydrogen separation from other light gases like CO2, N2, CH4, etc. is quite well known [32, 33]. In the first step and prior to membrane fabrication, SAPO 34 zeolite seed crystals were synthesized by hydrothermal technique, and characterization was done systematically to know the growth of SAPO 34 zeolite during hydrothermal process. The detailed studies on the gradual formation of SAPO 34 seed crystals at different times ranging from the initial gel mixture to 120 h at 170°C were described in our previous work [51]. The XRD pattern of the zeolite powders synthesized for 120 h is shown in Figure 5(a). The complete crystallization of SAPO 34 was noticed only after 120 h of hydrothermal synthesis at 170°C. All diffraction peaks are mostly similar to those of the chabazite structure of SAPO 34, and the d-values, i.e., (100), (110), (210), (220), (211), and (131), are in agreement with those reported in the literature [32]. Figure 5(b) shows the FESEM image of SAPO 34 seed crystals and almost all the crystals are cubical in nature having size 2-3 micron.
\n(a) XRD pattern of SAPO 34 zeolite synthesized by hydrothermal technique at 170°C for 120 h, (b) FESEM image of SAPO 34 zeolite, (c) bright field TEM image synthesized powder and inset show the EDS results, (d) corresponding SAED pattern of SAPO 34 zeolite, and (e) FTIR spectra of SAPO 34 zeolite samples synthesized at different time, ranging from 0 (initial gel mixture) to 120 h of hydrothermal synthesis [46, 51].
The TEM image of SAPO 34 powder after 120 h of hydrothermal synthesis is shown in Figure 5(c), which looks like a cubic structure, and corresponding SAED pattern reflected the CHA structure of SAPO 34 zeolite as shown in Figure 5(d). Figure 5(e) describes the FTIR spectra of the SAPO 34 zeolite powders collected at different time starting from 0 (initial gel) to 120 h, during seed synthesis by hydrothermal method. The various zeolitic vibration frequencies were assigned in accordance to the reported literature [1]. From this study, it was confirmed that after 120 h, the complete chabazite structure of SAPO 34 zeolite is formed. The characteristic band at 480, 534, and 568 cm−1 was attributed to the vibration of SiO4, (Si, Al) O4, and PO4, respectively. In addition, the vibration peak at 638 cm−1 matched with the double-6 rings (D6) would be the key evidence to CHA framework completeness. The gradual formation of SAPO 34 results at different time period, and the detail characterization was explained properly in the literature [51]. In the case of membrane synthesis, SAPO 34 zeolite membranes were synthesized on the clay-Al2O3 support by ex situ (secondary growth) hydrothermal method. In our approach we have prepared SAPO 34 zeolite membrane which is composed of three parts: the substrate, the intermediate layer, and the seed layer.
\nThe intermediate layer is composed of the polymeric/inorganic oxide layer with dispersed zeolite seed crystals. The importance of intermediate layer used for membrane synthesis was discussed in our reported results [40, 46, 47, 50]. The schematic representation for SAPO 34 membrane preparation is given here for better understanding (Figure 6).
\nSchematic representation of the different steps involved in SAPO 34 membrane syntheses.
In SAPO 34 membrane synthesis, silica intermediate layer was proposed for the selective deposition of oriented zeolite seed crystals with closely packed monolayers on a low-cost clay-Al2O3 tubular support and then subjected to the secondary growth under suitable hydrothermal conditions. As a result, a homogenous and reduced defect in highly oriented membrane can be synthesized simply. The organization of zeolite microcrystals with controlled orientation on substrates has been a subject of scientific interest, and recently, several approaches have been developed to prepare zeolite films with controlled orientation [52, 53, 54, 55].
\nSignificantly, using silica intermediate layer is predominantly based on the thermal and mechanical stability, as well as it being able to withstand in very high pressures. The silica surface under normal conditions is recovered with reactive hydroxyl groups, Si–OH, called silanol groups, and the high density of such surface –OH groups may promote high coverage of the resulting zeolite film and the highly oriented crystals. Furthermore, the implication of a silica layer plays an important role during membrane development. First of all, the layer helps to make the support surface smoother for the deposition of seed crystals in a uniform direction, and most importantly it acts as a blockade layer for the penetration of zeolite seed crystals into the interior of the support. Also it facilitates to persist the support layer with more hydroxyl (–OH) groups and as a result imparts the support with more nucleation points where crystals could bind on the support via van der Waals interactions and H-bonding [55]. In addition, it reduced stress-induced crack formation at the support–zeolite interface during calcination step [52]. The synthesized membranes were characterized by XRD, FESEM, and FESEM elemental mapping, etc. Finally the actual quality of the membrane was evaluated by gas permeation studies.
\nThe formation of phase pure SAPO 34 membranes with a high degree of crystallinity and correct orientation was confirmed by XRD analysis. Figure 7(a)–(d) shows the XRD patterns of the modified and nonmodified substrate, along with the membrane layer on that substrate. SAPO 34 membrane layer prepared on the nonmodified support shows that all diffraction peaks are most similar to those of the chabazite structure of SAPO 34, and the intensity of the peaks like (220), (211), (131), etc. are very much prominent which indicates the presence of pure SAPO 34 crystals from the membrane surface with random orientation.
\nXRD patterns of (a) bare support, (b) silica-modified support, (c) SAPO 34 membrane on the nonmodified support, and (d) membrane on the silica-modified support synthesized at 175°C for 120 h by hydrothermal process. (▪) peak from the clay-Al2O3 support [40].
In the case of XRD pattern of the SAPO 34 membrane prepared on the silica-modified support, a quite interesting result was perceived, that is, the intensity of the (210) peak which increases drastically compared with other peaks. It can be explained that the membrane developed towards higher orientation. In addition, the membrane layer also associates with small amount of non-oriented crystals [53]. The stronger intensity of the single peak proves the possibility of formation of an oriented membrane on the silica-modified support surface which plays a vital role in determining the high performance of the membrane. The same interpretation was noticed from the FESEM results. Figure 8(a) and (b) illustrates the FESEM micrograph of the bare support and silica-modified clay-Al2O3 support surface, respectively. The homogeneous oriented seed monolayer on the silica-modified support is shown in Figure 8(c). From the FESEM images, it can be explained that the majority of the seed crystals are deposited with proper orientation along with some disoriented seed particles interfering during the seeding process. Then during hydrothermal synthesis at 170°C for 120 h, the seed layer grows epitaxially and formed an oriented membrane layer on the support.
\nFESEM micrographs of (a) clay-Al2O3 substrate, (b) top view image of silica-modified support, (c) oriented seed monolayer on silica-modified support with a few misoriented seeds indicated by arrow marks, and (d) oriented SAPO 34 membrane layer synthesized on the seeded support prepared at 175°C for 120 h by a hydrothermal process [40].
\nFigure 8(d) depicts the surface morphology of the SAPO 34 membrane layers. It shows that the support surface was totally covered by uniform and compact cubic-shaped crystals, and no visible cracks, pinholes, or other macroscopic defects were observed. The FESEM micrograph of SAPO 34 membrane layer prepared on the nonmodified support surface has already been described earlier. The comprehensible discussion was described in our published paper [46]. This work is an attempt and is anticipated to have much importance for making defect-free low-cost highly oriented membranes which could offer to be a safe, simple, and environmentally benign potential application for gas separation application. Then ultimate gas separation performance of the SAPO 34 membrane is discussed to explain the membrane efficiency.
\nAlso another successful approach was implemented to develop an oriented defect-free membrane on the support surface. The oriented SAPO 34 membranes were grown on the support using a secondary (seeded) growth hydrothermal technique followed by insertion of 11-mercaptoundecanoic acid capped palladium (MUA-Pd) nanoparticles to the membrane.
\nPrior to membrane synthesis, first the clay-Al2O3 support was treated with polydiallyldimethylammonium chloride (PolyDADMAC) polymer, followed by deposition of seed layer homogeneously in a regular orientation on the support surface. A schematic representation of the membrane synthesis processes starting from bare support to nanoparticle insertion is shown in Figure 9. To deposit Pd NPs in the membrane matrix, a simple dip-coating technique was used. In practical, during thermal treatment of the Pd/SAPO 34 membrane, the instigation of defects is because of the removal of structure directing agent (SDA) from the zeolite pores. But interestingly, the presence of Pd NPs which entrapped inside the non-zeolitic pores and clogged the defects of the membrane. The synthesized membranes were characterized by XRD, TEM, XPS, and FESEM technique. FESEM and elemental mapping of the membrane cross section confirmed that most of the Pd NPs were deposited at the interface of the membrane and the support layer which may increase the membrane efficiency, i.e., separation efficiency.
\nSchematic representation of growth of SAPO 34 membrane starting from (a) bare substrate, (b) PolyDADMAC-modified layer to capture zeolite seed crystal, (c) seed monolayer onto the modified support, (d) synthesized membrane by secondary growth hydrothermal process, and (e) membrane layer decorated with MUA-capped Pd NPs [47].
The formation of phase pure, highly crystalline SAPO 34 zeolite on the support surface and the existence of Pd NPs on the membrane surface were confirmed by X-ray diffraction (XRD) patterns as revealed in Figure 10. From the XRD pattern of Pd/SAPO 34 membrane, it is clear that the intensity of the (210) peak is higher than other (100), (−110), (220), (211), and (−131) peaks and proves the presence of oriented crystals in the membrane layer. The Pd face-centered cubic phase has been identified from the Pd (111) peak which confirms the presence of Pd NPs in the membrane layer. The interpretation from the XRD results explained the presence of the Pd NPs, and the vital information is that the presence of Pd NPs did not affect the crystal structure of the SAPO 34 zeolite. It is because of the implicated nanoparticles which are too large to reside in the cavities (0.38 nm) of the framework. In general, during the heat treatment process, the structure directing agents (SDA) or any other organics are removed, and as a result, non-zeolitic pores, i.e., intercrystalline gaps, defects, or cracks, are formed.
\nXRD patterns of (a) clay-Al2O3 support, (b) the SAPO 34 membrane layer prepared on the nonmodified support, and (c) the Pd/SAPO 34 membrane layers on the modified support synthesized by the secondary growth hydrothermal technique [47].
Hence, it may be believed that the non-zeolitic pores were occupied by Pd NPs during the thermal treatment of the membrane, and further interpretation was established by FESEM studies, EDAX analysis, and elemental mapping. These results were explained in our earlier work [47]. For clear understanding, FESEM results were described here. Figure 11(a) depicts a FESEM micrograph of the Pd/SAPO 34 membrane layer prepared on the PolyDADMAC-modified support. It appears that a uniform membrane layer was formed with an interlocking structure. The uniformity of the membrane was achieved due to the coverage and proper orientation of seed crystals on the support which ultimately facilitated the formation of high-quality membrane. The high magnification FESEM data tells that no visible cracks, pinholes, or other macroscopic defects were noticed on the membrane layer. Then to know the membrane structure after thermal treatment, further FESEM characterization was done, and the micrograph of the calcined Pd/SAPO 34 membrane is illustrated in Figure 11(b). The membrane surface was analyzed carefully by selecting different areas. During inspection, the defective areas were identified, and to verify the presence of nanoparticles inside the defective area, EDAX analysis of the same area was done (Figure 11(c)). The Pd peak was identified along with SAPO 34 zeolite, and Si/Al ratio confirmed the complete growth of SAPO 34 zeolite. The quantitative elemental analysis of the synthesized Pd/SAPO 34 membrane coating is described in the table inset in Figure 11(c). The FESEM cross-sectional view (Figure 11(d)) shows that the thickness of the membrane is ~20–25 micron. The FESEM study revealed that the interlocked dense membrane was formed on the support surface successfully. However, the presence of Pd NPs which occupied and plugged into the non-zeolitic pores assisted towards the development of a nearly reduced defect membrane. It is noticed that two important phenomena were carried out simultaneously during thermal treatment. First, in the calcination process formation of non-zeolitic pores during the removal of structure directing agent, and simultaneously in the second step Pd NPs are migrating and entrapped inside the non-zeolitic pores and clogged the defects. Finally, in order to check the Pd/SAPO 34 membrane quality, gas permeation studies were carried out at room temperature in different feed pressures.
\nFESEM micrographs of (a) Pd/SAPO 34 membrane layer, (b) calcined Pd/SAPO 34 membrane (dotted circle indicated by arrow mark shows the defects formed after calcination processes), (c) corresponding EDS spectra taken from the selected area indicated by dotted circle and the inserted table show the quantitative analysis, and (d) cross-sectional view of the Pd/SAPO 34 membrane layer [47].
This work highlighted how the non-zeolitic pores of the synthesized membranes can be repaired by the insertion of palladium nanoparticles in the membrane matrix. Orientation and drastic reduction of non-zeolitic pores in the membrane layer may enhance the membrane quality for gas separation application.
\nHistorically, activated carbons and zeolites have been the most studied microporous materials (pore diameter < 2 nm) for the storage of gases. Zeolites were the first materials looked to as adsorbents for ANG technologies and methane adsorption in zeolites continue to assist in the understanding and design of adsorbent materials [57, 58]. Zeolites as hydrogen storage materials are investigated broadly, and it is found that small molecules such as molecular hydrogen can be easily absorbed into a flexible network of zeolites, and hydrogen adsorption properties of different types of zeolites have been investigated [59, 60, 61, 62, 63]. It was found that the amount of hydrogen adsorbed on zeolites can be affected by the framework composition, structure, charge-compensating cations, and acidic–basic nature. In order to create strong binding sites for H2 in zeolite pores, the importance of charge balance is quite inevitable. In this perspective, the role of light alkali metal cations such as Li+, Na+, and Mg2+ into the porous framework of zeolite plays an important role and enhances the binding energy for hydrogen adsorption [64]. Among the alkali metal cations (Li+, Na+, Mg2+), lithium ion is more capable due to its low atomic weight and high affinity towards hydrogen by charge-induced dipole interactions [65]. Based on this concept, Li substituted Bikitaite zeolite nanocrystals are synthesized at room temperature in short crystallization time by sonochemical method. Further, ultrasonic irradiations have been used along with hydrothermal treatment for synthesis of zeolite nanocrystals. First the synthesized powders were characterized by XRD and confirmed the gradual formation of highly crystalline material. Figure 12 shows the XRD pattern of sonochemically synthesized Bikitaite zeolite at different sonication time starting from 1.5, 2, and 3 h, and the sonication energy of 150 W was fixed for the synthesis. Before sonication, the sol was aged for 72 h at room temperature. The XRD result reveals that after 1.5 h sonication, the zeolite phase started forming and remained the same up to 3 h of irradiation. But complete growth of nanocrystalline Bikitaite phase was observed after hydrothermal treatment of sonicated sol for 24 h at 100°C. The figure clearly shows that the nanocrystalline Bikitaite zeolite with major peaks (100), (101), (201), etc. has formed and all the XRD patterns were compared with XRD pattern of simulated zeolite (COD file-969,003,103) as described in the literature [56]. Next, the morphology of the powders was observed by FESEM. Figure 12(b)–(e) depicts the morphology and corresponding EDAX analysis of the powders synthesized by only sonochemical method. Comparing these micrographs, it is clear that, at room temperature by ultrasonic irradiation, Li zeolite was formed with smaller size. But after further hydrothermal treatment, primary particles formed, reflecting porous woolen ball-like structures, which finally formed flake-like flower structure (Figure 12(d) inset).
\n(a) XRD pattern of Bikitaite zeolite synthesized with ultrasonic irradiation at different time, sonication energy of 150 W, aging time 72 h and sonication followed by hydrothermal treatment for 100°C and 24 h, FESEM micrograph of Bikitaite, prepared by (b) sonication for 3 h (inset: Higher magnified picture), (c) corresponding EDAX, (d) sonication followed by hydrothermal treatment at 100°C for 24 h (higher magnified picture is inset), and (e) corresponding EDAX [56].
The EDAX result (Figure 12(c) and (e)) explained that both phases show that the presence of silica is more than alumina which is in accordance to the reported stoichiometry of Bikitaite [66].
\nHydrogen adsorption capacity of the developed materials suited at cryogenic temperature and room temperature. The highest H2 adsorption capacity for pure Li zeolite reached up to 1.3 wt% which is more than the reported value. The synthesized zeolite was characterized by different techniques, and then the adsorption study carried out using appropriate method. The lithium doped sample showed higher hydrogen sorption capacity showed nearly 1.3 wt% compared with other zeolite as described in literature at 77 K and 1 bar pressure. Table 1 shows comparison of H2 adsorption capacity of Bikitaite with other reported values of zeolite [56]. The detailed study and explanation for hydrogen storage in Bikitaite zeolite have been discussed in our recent publication [67, 68].
\nComparison of H2 adsorption capacity of Bikitaite zeolite with reported values.
Finally, the study has shown that Bikitaite zeolite is a promising material for hydrogen storage. The storage volume increases with increasing Li content of the zeolite. This can be attributed by strong interaction between hydrogen molecule and high charge density of Li + ion. The detailed description of this work was reported earlier [56]. For membrane fabrication, the same powders were used as a seed for secondary growth. The mechanism and detailed procedure of membrane fabrication and their characterization results were discussed properly in the literature [69]. In this book chapter, only SAPO 34 and DDR membrane are highlighted.
\nIn this part gas permeation and separation studies of synthesized DDR and SAPO 34 membrane were discussed. In order to upgrade the quality of SAPO 34 zeolite membrane, different approaches have been taken as described previously. Successfully “reduced defect” or nearly “defect-free” oriented membranes were synthesized on the low-cost clay-Al2O3 support. The separation performances of the synthesized membrane designate whether a high-quality membrane was formed or not. Therefore the synthesized membranes were used for gas separation studies at different feed pressures as well as different feed compositions. The separation studies were carried out at room temperature.
\nIn the case of DDR membrane, the hydrogen separation efficiency was evaluated. Before gas permeation studies, the membranes were calcined to remove all the structure directing agents and organic compounds present in the zeolitic pore.
\nThe permeance is expressed as the flux rate through all the pores present in the membrane. The diffusion rate becomes significantly smaller where the kinetic diameter of the gas becomes larger than the pore size of the zeolite. The molecular kinetic diameters of H2 and CO2 are 0.29 and 0.33 nm, respectively, which are close to the pore size of DDR zeolite. The configurational diffusion and the variation in molecular size between H2 and CO2 result in the difference in the rate of diffusion through the DDR zeolite channels. The diffusion rate of H2 is faster than that of CO2, and therefore, H2 and CO2 can be separated by DDR zeolite membrane. Figure 13 describes the change of permeated flux of both H2 and CO2 through DDR zeolite membrane with varying transmembrane pressure difference. It shows that the rate of change of permeating flux with pressure is less for both CO2 and H2. In the case of molecular sieving through zeolitic pores, the rate of change of flux is pressure independent. But in this result, the little increase of flux with pressure shows that the membrane is associated with low concentration of non-zeolitic pores. At high pressure, CO2 adsorbs more strongly than H2 on the DDR zeolite membrane surface due to quadruple moment nature of CO2. So rate of desorption of CO2 from the membrane surface also decreases; as a result, permeating flux also decreases compared with hydrogen.
\nSingle gas permeated flux of H2 and CO2 as a function of transmembrane pressure difference [50].
The real performance of the membranes can be enlightened by their mixture gas separation ability. Figure 14 assigns the H2/CO2 separation factor of the mixture gas at room temperature as a function of CO2 feed concentration at 200 kPa feed pressure for the DDR membrane. From mixture gas, it is explained that selectivity decreases with increasing CO2 concentration. In general, CO2 has been preferentially adsorbed on the DDR pore surface, and therefore with increasing CO2 concentration, the extent of pore coverage has also increased. As a result, H2 permeability decreased and selectivity reduced spontaneously. The competitive adsorption-diffusion mechanism along with molecular sieving both is playing an important role for separation process. The H2/CO2 separation selectivity of the membrane increased up to 3.7 at room temperature which is more than the reported values and separation mechanism explained properly in our reported work [46].
\nH2/CO2 separation factor of the mixture gas at room temperature as a function of CO2 concentration in feed at 200 kPa feed pressure for DDR membrane [50].
But some appreciable gas separation results were found in the case of SAPO 34 membrane synthesized on SiO2 modified support. The SAPO 34 membrane synthesized on SiO2 modified support shows an appreciable hydrogen separation from CO2 and N2. Figure 15 shows the single gas permeation of H2 and CO2 at room temperature at different feed pressures. The synthesized membrane shows a relatively high hydrogen gas permeation value as compared with the literature values. Several factors might contribute to the higher hydrogen gas permeance through SAPO 34 zeolite membranes in this study. In general, the preferred orientation of the membrane layer plays a significant role in gas permeation. Generally, oriented porous paths exhibit superior performances compared with tortuous paths of randomly oriented pores of a membrane layer by minimizing the defect density and membrane resistance.
\nSingle gas permeation through SAPO 34 membrane at room temperature as a function of different feed pressures and separation selectivity of H2/CO2. The inset shows the comparison of separation selectivity of H2/CO2 by using SAPO 34 zeolite membrane prepared on the modified and nonmodified support surface [40].
Actually, in the case of a highly oriented membrane structure, the pores are more aligned, and the resistance of the gas transport through the aligned channel is less than that of the zigzag path of the nonaligned randomly oriented pores. As a result, membrane resistance decreases and the permeation adequacy enhanced, as compared with the randomly oriented membrane. As per our earlier discussion, the use of an intermediate silica layer which impedes the penetration of the zeolite seed particles inside the pores of the support increases the ultimate permeability of the membrane. So, combining all these aspects, it can be concluded that the almost defect-free, highly improved SAPO 34 membrane was developed on SiO2 modified support which shows higher hydrogen gas permeance with creditable results. The configurational diffusion and the difference in molecular size between H2 and CO2 result in a difference in the rate of diffusion through the SAPO 34 zeolite channels. The diffusion rate of H2 is faster than that of CO2. The H2/CO2 selectivity gradually increases with respect to the different feed pressures. More interestingly, at room temperature, the appreciable highest selectivity value for H2/CO2 was found to be 9.12. As shown in the inset of Figure 15, it describes the comparative study of selectivity for H2/CO2, and the values were lower through the SAPO 34 membrane prepared on the nonmodified support with respect to the modified support under different feed pressures. This result indicates that there are fewer non-zeolitic pores in the case of the SAPO 34 membrane on the modified support. However, the lowest selectivity values strongly indicate the presence of non-zeolitic pores, i.e., defects in the membrane layer.
\nThe real performance of the membranes can be investigated by their gas mixture separation ability (Figure 16). In the case of the H2/CO2 system, an appreciable selectivity value of 16.66 was obtained, and selectivity gradually decreased with increasing feed pressure. This phenomenon can be explained by the same way, i.e., an adsorption-diffusion model. At higher pressure, CO2 adsorbs more preferentially than H2 because it has the strongest electrostatic quadrupole moment, and more adsorption sites are generated which block some of the adsorptions of more weakly absorbing species. As CO2 adsorbs preferentially in the SAPO 34 pore wall, it also desorbs and diffuses earlier than H2, and the reasonable overall selectivity value in mixture was decreased. In H2-N2 gas mixture separation, a selectivity value of 20.91 was achieved and decreased to a small extent with respect to the feed pressures. Here, N2 has a negligible effect with respect to CO2 on H2 during the separation process, and because of the larger size of the N2 (0.36 nm) than CO2 (0.36 nm), the effect of molecular sieving plays a major role in the higher selectivity. The combined effect of these two determines the ultimate selectivity of the membrane. The obtained selectivity values are improved compared with the reported literature values as described in earlier data [40]. Fascinatingly, the selectivity values were performed at high values and remain almost constant up to 80 h. The high reproducibility was due to the formation of defect-free and highly oriented membrane layers.
\nRoom temperature separation selectivity of 50:50 H2/CO2 and 50:50 H2-N2 mixture as a function of different feed pressures. (flow rate = 100 mL min−1) [40].
Next, permeation results were given here to understand the Pd/SAPO 34 membrane quality. The flow rate of different gases was controlled by the mass flow controller (MFC). Figure 17 describes the single gas permeance of different gases through SAPO 34 membranes prepared on modified supports with and without Pd loading at 30°C and 200 kPa feed pressure as a function of the gas kinetic diameter (nm). It is interesting to note that single gas permeance through the Pd/SAPO 34 membrane at room temperature changed dramatically in comparison to the SAPO 34 membrane without Pd loading. As the kinetic diameter increased, the difference in the permeability of gases through those membranes decreased because of the difference in the kinetic diameter of gas molecule.
\nSingle gas permeances of different gases through SAPO 34 and Pd/SAPO 34 membranes prepared on modified supports at 30°C and 200 kPa feed pressure as a function of the gas kinetic diameter (nm) [47].
Mostly, the significant reduction of hydrogen permeance in the case of the Pd/SAPO 34 membrane as compared with the SAPO 34 membrane indicated the drastic reduction of non-zeolitic pores. However, in the case of the SAPO 34 membrane, the higher permeance value of H2 was obtained because of the presence of defects. From this result, it can be concluded that the non-zeolitic pores are at a minimum in the SAPO 34 membrane after Pd NPs loading. Figure 18 describes the change of single gas permeance of H2 and CO2 through the SAPO 34 and Pd/SAPO 34 zeolite membrane at different feed pressures. It can be explained that the rate of increase of the permeance values of CO2 with feed pressure is less than that of H2, and the explanation for this result has already been discussed. As CO2 adsorbs preferentially on the SAPO 34 zeolite membrane surface than H2, so the rate of desorption of CO2 from the membrane surface also decreased as compared with H2.
\nRoom temperature single gas permeation study of SAPO 34 and Pd/SAPO 34 membrane at different feed pressures. (flow rate 100 mL min−1) [47].
Hence, due to the preferential adsorption and diffusion of CO2 on the SAPO 34 zeolite surface and the difference in molecular size between H2 and CO2, there is a difference in the permeance values through the SAPO 34 zeolite channels.
\nAccording to Figure 18, as expected, the H2 permeability through the Pd/SAPO 34 membrane was lower than that through the SAPO 34 zeolite membranes, and the drastic reduction of the H2 permeance value as compared with SAPO 34 indicates that non-zeolitic pores were repaired by Pd NPs. Again, in the case of Pd/SAPO 34, the CO2 permeance values are almost equal at different feed pressures which confirm the removal of non-zeolitic pores and permeability through the Pd/zeolite membrane mainly due to the molecular sieving process which is less dependent on feed pressure.
\nThe real performance of the membrane for hydrogen gas separation from a mixture was evaluated from their mixture gas separation studies. The highest mixture gas separation factor for the Pd/SAPO 34 membrane was achieved at 20.8 [47]. However, the mixture separation factor in the case of the SAPO 34 membrane was 6.2. Both values, i.e., hydrogen permeation and separation factors, were higher than the literature values. Separation selectivity of the SAPO membranes increases appreciably after insertion of the Pd NPs which can reduce the non-zeolitic pores to a large extent and improve the membrane quality for hydrogen gas separation.
\nWe have summarized our ongoing research endeavors of microporous zeolite material for efficient gas storage and separation application. The key efforts that have been made mainly involve the synthesis of zeolite nanocrystal in a shorter crystallization time and develop the high-quality-oriented membrane on the low-cost support. To develop a high-quality membrane, different approaches have been taken and can be stated that our approach towards the development of high quality membrane is successful and may be applicable for other microporous materials for membrane development. The detail explanation and other fundamental understanding are described in our reported paper. Also many techniques are proposed by different research groups towards the development of ideal membrane and the clear understanding can be acquired from the literature. The hydrogen storage ability of Bikitaite zeolite is really commendable, and the H2 separation performance from H2-CO2 and H2-N2 mixture for DDR and SAPO 34 zeolite membrane is appreciable as compared with reported data. However, it should be noted that there are still many issues remaining to be addressed before implementation of industrial and commercial usage of these developed materials for separation and storage purpose. For these issues, chemists and engineering scientists of different expertise and industrial partners need to work cooperatively. In realistic separation systems, the gas mixtures and operation conditions are more complicated, and many factors need to be taken into account to perform successfully under industrial relevant condition. There is no doubt that zeolite materials are an area of great excitement and potential importance in all the areas. It would be a great achievement for such materials to be applied in practice.
\nThe authors would like to thank CSIR, India, and also thankful to Dr. K Muraleedharan, Director, CSIR-CGCRI, for his kind permission to publish the book chapter.
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\n'}]},successStories:{items:[]},authorsAndEditors:{filterParams:{sort:"featured,name"},profiles:[{id:"6700",title:"Dr.",name:"Abbass A.",middleName:null,surname:"Hashim",slug:"abbass-a.-hashim",fullName:"Abbass A. Hashim",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/6700/images/1864_n.jpg",biography:"Currently I am carrying out research in several areas of interest, mainly covering work on chemical and bio-sensors, semiconductor thin film device fabrication and characterisation.\nAt the moment I have very strong interest in radiation environmental pollution and bacteriology treatment. The teams of researchers are working very hard to bring novel results in this field. I am also a member of the team in charge for the supervision of Ph.D. students in the fields of development of silicon based planar waveguide sensor devices, study of inelastic electron tunnelling in planar tunnelling nanostructures for sensing applications and development of organotellurium(IV) compounds for semiconductor applications. I am a specialist in data analysis techniques and nanosurface structure. I have served as the editor for many books, been a member of the editorial board in science journals, have published many papers and hold many patents.",institutionString:null,institution:{name:"Sheffield Hallam University",country:{name:"United Kingdom"}}},{id:"54525",title:"Prof.",name:"Abdul Latif",middleName:null,surname:"Ahmad",slug:"abdul-latif-ahmad",fullName:"Abdul Latif Ahmad",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"20567",title:"Prof.",name:"Ado",middleName:null,surname:"Jorio",slug:"ado-jorio",fullName:"Ado Jorio",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Universidade Federal de Minas Gerais",country:{name:"Brazil"}}},{id:"47940",title:"Dr.",name:"Alberto",middleName:null,surname:"Mantovani",slug:"alberto-mantovani",fullName:"Alberto Mantovani",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"12392",title:"Mr.",name:"Alex",middleName:null,surname:"Lazinica",slug:"alex-lazinica",fullName:"Alex Lazinica",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/12392/images/7282_n.png",biography:"Alex Lazinica is the founder and CEO of IntechOpen. After obtaining a Master's degree in Mechanical Engineering, he continued his PhD studies in Robotics at the Vienna University of Technology. Here he worked as a robotic researcher with the university's Intelligent Manufacturing Systems Group as well as a guest researcher at various European universities, including the Swiss Federal Institute of Technology Lausanne (EPFL). During this time he published more than 20 scientific papers, gave presentations, served as a reviewer for major robotic journals and conferences and most importantly he co-founded and built the International Journal of Advanced Robotic Systems- world's first Open Access journal in the field of robotics. Starting this journal was a pivotal point in his career, since it was a pathway to founding IntechOpen - Open Access publisher focused on addressing academic researchers needs. Alex is a personification of IntechOpen key values being trusted, open and entrepreneurial. Today his focus is on defining the growth and development strategy for the company.",institutionString:null,institution:{name:"TU Wien",country:{name:"Austria"}}},{id:"19816",title:"Prof.",name:"Alexander",middleName:null,surname:"Kokorin",slug:"alexander-kokorin",fullName:"Alexander Kokorin",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/19816/images/1607_n.jpg",biography:"Alexander I. Kokorin: born: 1947, Moscow; DSc., PhD; Principal Research Fellow (Research Professor) of Department of Kinetics and Catalysis, N. Semenov Institute of Chemical Physics, Russian Academy of Sciences, Moscow.\r\nArea of research interests: physical chemistry of complex-organized molecular and nanosized systems, including polymer-metal complexes; the surface of doped oxide semiconductors. He is an expert in structural, absorptive, catalytic and photocatalytic properties, in structural organization and dynamic features of ionic liquids, in magnetic interactions between paramagnetic centers. The author or co-author of 3 books, over 200 articles and reviews in scientific journals and books. He is an actual member of the International EPR/ESR Society, European Society on Quantum Solar Energy Conversion, Moscow House of Scientists, of the Board of Moscow Physical Society.",institutionString:null,institution:{name:"Semenov Institute of Chemical Physics",country:{name:"Russia"}}},{id:"62389",title:"PhD.",name:"Ali Demir",middleName:null,surname:"Sezer",slug:"ali-demir-sezer",fullName:"Ali Demir Sezer",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/62389/images/3413_n.jpg",biography:"Dr. Ali Demir Sezer has a Ph.D. from Pharmaceutical Biotechnology at the Faculty of Pharmacy, University of Marmara (Turkey). He is the member of many Pharmaceutical Associations and acts as a reviewer of scientific journals and European projects under different research areas such as: drug delivery systems, nanotechnology and pharmaceutical biotechnology. Dr. Sezer is the author of many scientific publications in peer-reviewed journals and poster communications. Focus of his research activity is drug delivery, physico-chemical characterization and biological evaluation of biopolymers micro and nanoparticles as modified drug delivery system, and colloidal drug carriers (liposomes, nanoparticles etc.).",institutionString:null,institution:{name:"Marmara University",country:{name:"Turkey"}}},{id:"61051",title:"Prof.",name:"Andrea",middleName:null,surname:"Natale",slug:"andrea-natale",fullName:"Andrea Natale",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:null},{id:"100762",title:"Prof.",name:"Andrea",middleName:null,surname:"Natale",slug:"andrea-natale",fullName:"Andrea Natale",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"St David's Medical Center",country:{name:"United States of America"}}},{id:"107416",title:"Dr.",name:"Andrea",middleName:null,surname:"Natale",slug:"andrea-natale",fullName:"Andrea Natale",position:null,profilePictureURL:"//cdnintech.com/web/frontend/www/assets/author.svg",biography:null,institutionString:null,institution:{name:"Texas Cardiac Arrhythmia",country:{name:"United States of America"}}},{id:"64434",title:"Dr.",name:"Angkoon",middleName:null,surname:"Phinyomark",slug:"angkoon-phinyomark",fullName:"Angkoon Phinyomark",position:null,profilePictureURL:"https://mts.intechopen.com/storage/users/64434/images/2619_n.jpg",biography:"My name is Angkoon Phinyomark. I received a B.Eng. degree in Computer Engineering with First Class Honors in 2008 from Prince of Songkla University, Songkhla, Thailand, where I received a Ph.D. degree in Electrical Engineering. My research interests are primarily in the area of biomedical signal processing and classification notably EMG (electromyography signal), EOG (electrooculography signal), and EEG (electroencephalography signal), image analysis notably breast cancer analysis and optical coherence tomography, and rehabilitation engineering. I became a student member of IEEE in 2008. During October 2011-March 2012, I had worked at School of Computer Science and Electronic Engineering, University of Essex, Colchester, Essex, United Kingdom. In addition, during a B.Eng. I had been a visiting research student at Faculty of Computer Science, University of Murcia, Murcia, Spain for three months.\n\nI have published over 40 papers during 5 years in refereed journals, books, and conference proceedings in the areas of electro-physiological signals processing and classification, notably EMG and EOG signals, fractal analysis, wavelet analysis, texture analysis, feature extraction and machine learning algorithms, and assistive and rehabilitative devices. I have several computer programming language certificates, i.e. Sun Certified Programmer for the Java 2 Platform 1.4 (SCJP), Microsoft Certified Professional Developer, Web Developer (MCPD), Microsoft Certified Technology Specialist, .NET Framework 2.0 Web (MCTS). 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